Composition of matter and method for making the same



Patented June 1, 192 6.

UNITED STATES CROSS (I? Bil-MINER PATENT OFFICE.

mm W. mm, 01 IBIEPOBT, nw YORK, ABSIG NOB TO r'maur. SYNDICATE LTD, 01' BROOKLYN, m YORK, A CORPORATION 01 II'GLAI'D.

OOITOSITION O1 ua'r'rnn um n'rnon 103 name rm: BAD.

Io Drawing.

This invention relates to a composition-of matter and a method for making the same. More particularly the invention comprises 'a composite product from fused silica or I fused quartz and a method for the production thereof.

As is-well known silica exists in a large variety of forms having very different properties. Ordinary sand, for example, is Sillcon dioxide-or s1lica, SiO,, and is a crystalline form thereof. Ordinary quartz, also known as rock crystal, is a crystalline rhombohedral form 0 silica having substantially the same perzperties as ordinary sand.

It has 11 found that when quartz is fused in the oxyhydrogen flame or in the electric and cooled, a material is obtained of the same composition as quartz but having widely difierent physical prop erties, the resultant materia having very low coeflicient of expansion and can therefore be heated or cooled as suddenly as desired without risk of fracture. It is apparent that the new gllysical properties result from a change in p ysical state, the material being it is generally assumed, in the form of a supercooled liquid.

I have found that by treating fused quartz according to the method hereinafter fully 10 disclosed a product is obtained which, while retaining the desirable characteristics of low expansion with heat and high dielectric stre th, possesses certain valuable properties ermg from those of the original 85 fused quartz whereby it is adapted or 'a variety of uses for which the ori material cannot be employed.

Fused quartz or fused silica has become during recent years, an important article of 40 commerce being employed for chemical equipment, electrical ap aratus, and for articles of all kinds in w 'ch the material is subjected to extreme temperature char-ifs The various articles made from fused 'ca frequently become broken and are merely thrown to waste no commercial means having been de for utilizing such broken fused quartz material.

The resent invention has for an object the u ation -of waste or crushed fused silica or fused qluartz by the production of a new and usefu product therefrom. Another object of the invention is to provide a process whereby the fused quartz or 'i ix.

Application fled I87 3, 1935. Serial 10. 88,874.

fused silica may be treated to attain the de- N sired roduct.

Wit these and other objects in view the invention comprises the various features hereinafter more fully described and particularly defined in the claims.

In order to carry out my invention, I preferably comminute fused silica or fused quartz to asuitable state of sub-division, either by grinding, or crushing, or by any other suitable method. This und fused silica is then mixed with a cient amount of a sodium silicate solution, so as to form a stiff paste, and is then molded into any desired form, for the production of plates, rods, bricks or other articles to be made 7 therefrom I preferably employ equal proportions by weight of pure ground fused silica of 20 and 150 mesh fineness and admix therewith a solution of sodium silicate.

Various forms of solutions are suitable for my purpose, the particular strength or form of solution to be employed depending on the state of sub-division of the fused quartz or fused silica employed and also upon the particular results desired, as for .0 example, where certain particular pro rties are desired in the final product w 'ch is to be applied to a special use, or depending upon other factors as will be apparent to those skilled in the art. I may employ 86 a saturated solution of sodium silicate, for example, although I preferably employ a solution havin the following composition which I have time best suited for my pur- I r a .0-

C an SiO, 24.7 Na,0 6.4 11,0 68. 9

The above composition corresponds substiantizll go 6 saturaged solution off wtaoter gass a,'i,,an asa vityoaut 37 Baum at 68 F. It igte be understood, however, that this composition as above set forth, is given only for purposes of illustrating the composition which I have found best suited under ordinary conditions for the production of m product and that I do not desire to be imited to this composition. Any solution ha 'an uivalent action, such as a solution 0 the a ve composition which has been diluted or a solution in which the ratio of SiO, to

' the acid from about five to ten hours, al

Na,O is less than the above, or a solution in which potassium silicate is substituted as a whole or in part for sodium silicate, may be em loyed in place of the above.

'Fbe amount of the silicate solution which is to be employed in admixture with the fused silica or, in other words, the roportion of solution to the dry powdere mate- .rial, will vary with the fineness of grinding of the silica material and upon the proportions of the various grades of fineness of the fused silica which is employed. The requisite or suitable amount of solution for a given amount of fused silica material may be readily determined by means of a trial sam le, as will be apparent to those skilled in t e art, or the amount may be read ly determined if desired, through observation or tests during the mixing process of the solution with the ground silica mater al. While I prefer to carry out my invention by mixing the powdered fused silica or quartz material of the grades of fineness, as above set forth, it is obvious that powdered material of other grades ma beemployed or a mixture of a number of ifierent grades may be used, if desired. On the other hand, I may employ for special purposes, fused silica or quartz powder .of 'a single ade of fineness as, for example, where uni ormity of structure in the material is desired.

After the silica material and silicate solution have been pro erly mixed to form a paste of the desi consistency, the material is transferred to a suitable mold or molds, whereby the material is shaped into whatever form is desired in the final prodnot.

After the material has been molded to the desired form, either under presure or without ressure, it is allowed to dry. for several ays at any suitable temperature. This is preferably accomplished at ordinary room temperature although a higher or lower temperature may be used.

After the material has set for a sufiicient length of time a strong bond is produced between the various particles of the compontion which, it is believed, may be due to a reaction between the ingredients of the composition. The molded o ject, after the above treatment, is immersed in concentrated hydrochloric acid for a suflicient length of time to cause a separation of silicic acid from sodium silicate within the pores of the material, the objects being allowed to remain in though a shorter or longer time may be employed, depending on the sizeof the obects, the strengt of the acid, and other considerations as will be apparent to those skilled in the art. It is not definitely known what reaction takes place through this treatment, although it appears that silicic acid is separated out in the process and is diatributed through the pores of the material. After the acid treatment the object is washed to remove the remaining acid.

If desired the excess acid adhering to the object may be removed by a preliminary treatment with water and, thereafter, the remainder of the acid may be neutralized with ammonia, which is preferably employed in a pure concentrated form. The ammonia, or ammonium hydroxide reacts with the hydrochloric acid present to form ammonium chloride, which may be readily washed out, but does not react with the se arated silicic acid. If ammonia is em loy in the rocess the soluble salts which are form are preferably removed by washing the obiect in running water for a period of not ess than twelve hours, the time of treatment bemg, of course, dependent upon the nature and size of the ob ect.

After the object has been treated for a suflicient length of time'in the water, as may be determined by testing a sample of the water in contact therewith by means of indicators or other chemical tests to determine the int at which the water soluble material has n removed, the object is dried, either in the air or in an oven.

, After the treatment with water, the silicic acid, which has been introduced into the object and liberated within the pores thereof from sodium silicate is apparently in an amo hous form. The exact form in which the silicic acid exists in my new composition of matter is not known entirel for the reason that there are man difi'erent drated forms of silicic acid, w 'ch in com ination with other material are extremel diflicult to identify, or which it is substantially impossible to :ieparate without changing their composi- It is well known that the ortho-silicic acid Si( OH) breaks down b liberation of water into the metasilicic aci H,SiO,, and into disihcic acids, such as H,Si,0,, for example, and further to trisilicic acid H,Si,0,. It seems robable that in my composition several 0 these various forms are present and actasahindingmaterial.

I that my product has very valuable properties which are not resent in the original fused silica employ Fused silica,

.for example, has a limited field of use on account of the dificulty involved in forming the various desired aha while in the state of fusion, and only sun is forms can be made on a commercial scale.

I have found, however, that by using the method above described a material is obtained which has substantially the same low coeficient of expansion and high chemical co as fused silica or fused uartz, and has the additional advantage t it may be molded into substantially any desired shape and is adapted, therefore, for

the production of insulating members, apparatus of com licated forms, and for 0 uses for whic fused if a colored mIateria ot er u ose, ma inco rate a filing material iiiadd othe i' inert iiaterial whic will not interfere with the particular use to which the ob'ect is to be put. I may also, if desired, pr uce a surface glaze on the material, thus increasing its tensile strength, as by incipient surface fusion, for example, which may -be attained by subject' the body to a sufiicient degree of heat, or may impre ate the product with any suitable material such as parafin or other medium which is adalpted to enter the pores of the product, or

quartz is unsuited.

is desired, or for any terial to suitably modify the appearance of the product, and to adapt it to other uses, such as radio apparatus for example.

It is to be un erstood that I do not desire to be limited as to the form of the silicic acid in my product which may be either in the hydrated or substantially dehydrated form. It is to be understood, furthermore, that various changes and modifications may be made in the product and the method above described without departing from the spirit and scope of the invention as defined in the claims.

Havirg thus described the invention, what is claim as new is:

1. An article of manufacture comprising comminuted fused silica and silicic acid.

2. A composition of matter comprising a molded mixture of fused silica and silicic acid in combination therewith.

3. An article of manufacture comprisigg fused and hydrated silica combin therewith as a cementing medium.

4. An article of manufacture comprising fused silica and a cementing medium obmay cover the surface of the object with varnish or other insulating ma-- tained by admixing with fused silica an alkaline silicate solution to form a paste, molding the said paste, treating with a strong acid, and drying the mass.

5. An article of manufacture comprising the resultant roduct obtained by treatment of comminuted fused silica with sodium silicate to form a aste therefrom, molding the said paste to t e desire form, treating the molded mass with concentrated hydrochloric acid to liberate silica from the said silicate, removing the excess of hydrochloric acid, thereafter treating the molded mass with ammonia, washing out the soluble salts therefrom with water, and drying the molded mass.

6 A rocess for the utilization of waste fused SHlCB. which com rises comminuting fused silica, adding a so uble silicate thereto to form a paste, molding the product thereof, treating the said roduct with a stron acid to liberate SlllClO acid from the sai soluble silicate within the body of the said molded product and thereafter removing the said acid and dr ing the product.

7. A rocess for t e utilizationof waste fused s1 ca which comprises comminuting fused silica, mixing a sodium silicate solution therewith to form a paste, molding the paste into a body of the desired form, drying the molded body, treating the said body with a concentrated h drochloric acid solution for a sufiicient time to attain the desired reaction, removing the excess of acid from the said body treating the said bod with ammonia, washing the said body wit water for a suflicient time to remove soluble salts from the said body, and finally drying the said body Signed at New York city, N. Y., this 4th day of May, 1925. H

WILLIAM w, wmsmr. 

